m-Chloroperbenzoic acid → HCID 178493774, 화합물

HRID 845514노트

반응식

HRID 845514 반응식
[CH3:1][O:2][C:3]1[C:8]([O:9][CH3:10])=[CH:7][N:6]=[C:5]([CH2:11][S:12][C:13]2[NH:17][C:16]3[CH:18]=[CH:19][C:20]([O:22][C:23]([F:28])([F:27])[CH:24]([F:26])[F:25])=[CH:21][C:15]=3[N:14]=2)[CH:4]=1.ClC1C=C(C=CC=1)C(OO)=[O:34]>C(Cl)Cl>[CH3:1][O:2][C:3]1[C:8]([O:9][CH3:10])=[CH:7][N:6]=[C:5]([CH2:11][S:12]([C:13]2[NH:17][C:16]3[CH:18]=[CH:19][C:20]([O:22][C:23]([F:27])([F:28])[CH:24]([F:25])[F:26])=[CH:21][C:15]=3[N:14]=2)=[O:34])[CH:4]=1

참가 물질

4

반응물 2

HCID 70297m-Chloroperbenzoic acidHCID 178493768HCID 178493768, 화합물

생성물 1

HCID 178493774HCID 178493774, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

A solution of the product in methylene chloride is obtained by the procedure described in Example 2 by oxidation of 0.76 g of 2-[(4,5-dimethoxy-2-pyridyl)methylthio]-5-(1,1,2,2-tetrafluoroethoxy)-1H-benzimidazole with 19 ml of a 0.1M solution of m-chloroperoxybenzoic acid in 30 ml of methylene chloride at -40° C., after extraction. After drying the solution over magnesium sulfate, the drying agent is filtered off, the filtrate is concentrated and the residue is crystallized from methylene chloride/diisopropyl ether. 0.64 g (82% of theory) of the title compound is obtained in the form of colorless crystals of m.p. 160°-162° C. (decomp.).

후처리

  1. extractionafter extraction
  2. dry with materialAfter drying the solution over magnesium sulfate
  3. filtrationthe drying agent is filtered off
  4. concentrationthe filtrate is concentrated
  5. customthe residue is crystallized from methylene chloride/diisopropyl ether

출처 및 근거

ORD 기록
ord-fb452fa10f6f47d1b71b3a9855095567
출처 데이터셋
uspto-grants-1988_07
특허 번호
US04758579

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